反应详情

温度

0 °C

To a suspension of sodium hydride (1.2 mmol) in DMF (6 mL), 4-chloro 3-methyl 6-nitrophenol (1.0 mmol) was added at 0° C. The reaction mixture was stirred at 0° C. for 15 minute then methyliodide was added at 0° C. and the mixture was stirred for 4 hours at room temperature. Water (60 mL) was added and the mixture extracted with EtOAc (3×50 mL). The combined organic extracts were washed with water (50 mL), brine (50 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by column chromatography on silica using 5-8% EtOAc in hexane to give the title compound (87%) as a solid.

1. additionwas added at 0° C
2. stirringthe mixture was stirred for 4 hours at room temperature
3. extractionthe mixture extracted with EtOAc (3×50 mL)
4. washThe combined organic extracts were washed with water (50 mL), brine (50 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by column chromatography on silica using 5-8% EtOAc in hexane